CN206276369U - A kind of association response device of glyoxal oxidation synthesis glyoxylate - Google Patents
A kind of association response device of glyoxal oxidation synthesis glyoxylate Download PDFInfo
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- CN206276369U CN206276369U CN201620590366.3U CN201620590366U CN206276369U CN 206276369 U CN206276369 U CN 206276369U CN 201620590366 U CN201620590366 U CN 201620590366U CN 206276369 U CN206276369 U CN 206276369U
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- glyoxal
- association response
- response device
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- oxidation synthesis
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Abstract
The utility model discloses a kind of association response device of glyoxal oxidation synthesis glyoxylate, belong to technical field of chemical, it includes：Reactor, nitric acid adds pipe, circulating pump, gas-liquid reactor, air intlet, reacting pipe, external heat exchanger, reflux condenser, sample tap, glyoxalic acid is exported, a kind of association response device of the such as tail gas absorber synthesizing glyoxalic acids of the present utility model, it is little with investment, install easy, easy temperature control system, low power consumption and other advantages association response devices of the present utility model participate in reaction by introducing air, by reactor, reacting pipe, gas-liquid reactor, the close fit of external heat exchanger, so that glyoxal obtains larger raising to the conversion ratio and glyoxalic acid quality of glyoxalic acid.
Description
Technical field
The utility model belongs to technical field of chemical, is related to a kind of reaction unit of glyoxal oxidation synthesis glyoxylate,
More particularly to a kind of glyoxal nitric acid oxidation method, air participate in the association response device of the synthesizing glyoxalic acid of oxidation.
Background technology
Glyoxalic acid is important fine chemical material, is widely used in the industries such as spices, pharmacy, agricultural chemicals, chemical industry.
Glyoxal nitric acid oxidation method synthesizing glyoxalic acid is the technique of the production glyoxalic acid that most domestic enterprise uses.The work
The advantage of skill is that the small, cost of investment is relatively low.
The chemical equation of glyoxal nitric acid oxidation method synthesizing glyoxalic acid is as follows：
3CHO-CHO + 2HNO3→ 3CHOCOOH + 2NO↑+ H2O
At present, the open defect of glyoxal nitric acid oxidation method synthesizing glyoxalic acid technique shows as following several respects
The glyoxal of about equivalent 17 ± % is excessively oxidated and is converted into our unwanted oxalic acid, its chemical reaction
Equation is as follows：
3CHOCOOH + 2HNO3→3COOH-COOH + NO↑+H2O
During tail gas absorption, due to the effect of vacuum and entrained liquid, the equivalent 4-6% glyoxals that there are about enter absorption
Tower is consumed by nitric acid.
The reaction of glyoxal nitric acid oxidation method synthesizing glyoxalic acid is strong exothermal reaction, and the heat exchange area of reacting kettle jacketing only has
15m2Left and right, cooling-down effect can not meet oxidation reaction heat release the need for therefore, reaction temperature be difficult to control.
Air has been only involved in tail gas absorption reaction, is not engaged in the oxidation reaction of glyoxal, and this objectively increased nitre
The consumption of acid, increases the quantum of output of accessory substance oxalic acid.
For the defect in current glyoxal nitric acid oxidation method synthesizing glyoxalic acid technique, we pass through further investigation, into
Work(develops a kind of glyoxal oxidation technology technology and oxidation unit that can reduce disadvantages described above.
The content of the invention
The utility model provides a kind of association response device of oxidation of glyoxal synthesizing glyoxalic acid, it is characterised in that
1. reaction temperature can be precisely controlled, 2. air can participate in the oxidation reaction of glyoxal, 3. conversion of the glyoxal to glyoxalic acid
Rate is highly improved.
A kind of association response device of glyoxal oxidation synthesis glyoxylate that the utility model is provided, it includes：Reactor,
Nitric acid adds pipe, circulating pump, gas-liquid reaction device, air intlet, reacting pipe, external heat exchanger, circulation water entrance, backflow
Condenser, cool brine import and export, sample tap, glyoxalic acid outlet, tail gas absorber, it is characterised in that gas-liquid reaction device one end leads to
Cross circulating pump to be connected with reactor bottom, the other end of gas-liquid reaction device is connected by external heat exchanger with reactor top,
The side import of gas-liquid reaction device and air communication.
Preferably, the reactor described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model
Chuck is only connected with jet chimney, and it is only used for heating in reaction of the present utility model.
Preferably, the nitric acid described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model adds
Enter pipe port and add homemade at the uniform velocity Dropping feeder.
Preferably, the solution-air described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model
Reactor is enamel, PP or F4Material, its main diameter is 80-200mm, and port is connected with fluid accelerating attachment.
Preferably, the air described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model enters
Mouth connection self-control air purifier.
Preferably, the reaction tube described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model
Road is PP, F4Or enamel material, its length is 5.0-25.0m.
Preferably, the outer displacement described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model
Hot device is graphite, glass material heat exchanger, and heat exchange area is 10-80m2, it circulates water entrance and is connected with 25 °C of ± recirculated waters.
Preferably, the returned cold described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model
Condenser is coil pipe type glass condenser, and area is 1.5-15.0m2, it condenses the cool brine that water entrance is connected with 5-15 °C.
Preferably, the tail gas described in a kind of association response device of glyoxal oxidation synthesis glyoxylate of the present utility model is inhaled
Receipts tower is PP materials, built-in spherical PE fillers or ripple packing, is combined as an absorption tower by the series connection of 2-8 platforms absorption tower.
A kind of association response device of glyoxal oxidation synthesis glyoxylate that the utility model is provided and glyoxal before
Oxidation reaction apparatus compare, with following clear advantage：
1. the at the uniform velocity addition of nitric acid, it is to avoid hot-spot phenomenon.
2. reaction solution is heated by reacting kettle jacketing, reaction solution is lowered the temperature by external heat exchanger, heat is cold
Lock out operation is more conducive to the control of temperature.
3. gas-liquid reaction device can make air continuously enter the oxidation reaction that reaction solution participates in glyoxal, Jin Erhui
Mild reaction conditions, reduction nitric acid unit consumption, it is possible to increase the conversion ratio of glyoxal to glyoxalic acid.
4. reaction of the reaction solution after acceleration in the reacting pipe of relative closure can more fully, and this is to improving glyoxal
Conversion ratio is highly beneficial.
5. by increasing reflux condenser heat exchange area, to the method for the logical cool brine of reflux condenser so that solution-air is carried secretly
Glyoxal and glyoxalic acid drop and return to reactor, meanwhile, absorption tower is more beneficial for through the reaction end gas after cooling and reclaims dilute nitre
Acid.
A kind of such device, the association response device of glyoxal oxidation synthesis glyoxylate that the utility model is provided makes
Reaction temperature it is easily controllable while, additionally it is possible to nitric acid unit consumption is decreased, the conversion ratio of glyoxal to glyoxalic acid have compared with
It is big to improve.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of the association response device of glyoxal oxidation synthesis glyoxylate of the present utility model.
Specific embodiment
To make device of the present utility model, technical scheme clearly express, below in conjunction with the accompanying drawings to the utility model
Carry out in detail, be fully described by obviously, described embodiment is a part of embodiment of the present utility model, and not all.
This specific embodiment embodiment provides a kind of association response device of oxidation of glyoxal synthesizing glyoxalic acid, its
It is characterised by, including：1- nitric acid adds pipe, 2- other raw materials additions pipe, 3- nitric acid droppings port, 4- steam inlets, 5- reactions
Kettle main body, the outlet of 6- steam drainages, 7- reacting kettle jacketings, 8- reflux condensers, the import of 9- cool brines, 10- cool brines outlet,
11- circulating pumps, 12- gas-liquid reactions device, 13- air intlets, 14- external heat exchangers, 15- circulating water intakes, 16- recirculated waters go out
Mouth, 17- sample taps, 18- products exports, 19- absorption towers combination, 20- can emission outlet etc..
The detailed process of this specific embodiment embodiment is as follows：First the glyoxal needed for reaction, composite catalyst are pressed
Ratio adds reactor -5, starts stirring, starts circulating pump -11, makes reaction solution in gas-liquid reaction device -12, reacting pipe, outer
Put and circulated between heat exchanger -14, reactor -5, to being passed through steam in reacting kettle jacketing -4, reacted during uniform temperature and started, matching somebody with somebody
Be made certain density dust technology adds pipe -1 and nitric acid dropping port -3 at the uniform velocity to add the reaction end gas of reactor -5. by nitric acid
After being condensed through reflux condenser -8, a part condenses back into reactor, and another part changes into dilute nitre into absorption tower combination -19
Acid, tail gas after absorption through in the discharge reaction solution cyclic processes of offgas outlet -20, air by gas-liquid reaction device -12 in a steady stream
After the oxidation reaction for constantly participating in glyoxal into reaction solution is reacted to certain hour, quick detection is sampled from sample tap -17
Glyoxal is remaining, when glyoxal remnants reach requirement, product is transferred to product storage tank through products export -18.
Such device, a kind of association response of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Device, by controlling the feed postition of nitric acid, enable nitric acid at the uniform velocity to add, it is to avoid hot-spot phenomenon, and then reduces
The yield of accessory substance oxalic acid.
Such device, a kind of association response of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Device, described reacting kettle jacketing is only used for heating reaction solution, and external heat exchanger is only used for lowering the temperature reaction solution,
The cold lock out operation of heat is more beneficial for the control of temperature, it is to avoid the fluctuation bounce of temperature, and this is highly beneficial to oxidation reaction.
Such device, a kind of association response of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Device, described gas-liquid reaction device can make air continuously enter the oxidation reaction that reaction solution participates in glyoxal, Jin Erhui
Mild reaction conditions, reduction nitric acid unit consumption, the conversion ratio of raising glyoxal to glyoxalic acid.It is anti-after accelerating through gas-liquid reaction device
Answer reaction of the liquid in the reacting pipe of relative closure more abundant, this is to improving conversion ratio, reduction of the glyoxal to glyoxalic acid
Oxalic acid quantum of output is highly beneficial.
Such device, a kind of association response of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Device, by increasing reflux condenser heat exchange area, to the method for the logical cool brine of reflux condenser so that the second of solution-air entrainment
Dialdehyde and glyoxalic acid drop and return to reactor, at the same be more conducive to through the reaction end gas after cooling absorption tower reclaim nitric acid this to subtracting
It is few glyoxal loss, highly beneficial to the absorption of nitric acid.
As preferred and citing, a kind of connection of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Close the cooling water that is passed through of external heat exchanger involved by reaction unit can be 25 °C ± recirculated water, but, returned cold
The cooling water that condenser is passed through must be less than 15 °C of cool brine.
As preferred and citing, a kind of connection of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Gas-liquid reaction device involved by reaction unit is closed, its operating pressure is 0.01-0.03Mpa, therefore it is required that gas-liquid reaction device pressure-bearing
0.05Mpa。
As preferred and citing, a kind of connection of glyoxal oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Close tail gas absorber combination involved by reaction unit, be made up of 2-8 platforms absorption tower, the vavuum pump of its end only play drainage and
Negative pressure can not be shown.
A kind of implementation result of association response device of glyoxal oxidation synthesis glyoxylate that the utility model is provided is：
While so that reaction temperature is easily controllable, additionally it is possible to nitric acid unit consumption is decreased, the conversion ratio of glyoxal to glyoxalic acid reaches
To 83.0-87.0%, simultaneously as the reduction of oxoacetic acid product mesoxalic acid and other organic by-products amounts, to other follow-up works
Sequence is highly beneficial.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or new using this practicality
Various modifications that type is carried out to these embodiments, will be apparent for professional and technical personnel, determine herein
Justice General Principle can in other embodiments be realized in the case where spirit or scope of the present utility model are not departed from, because
This, the utility model will not be limited to the embodiments shown herein, every within the utility model spirit and principle,
Any modification, equivalent substitution and improvements made etc., should be included within protection domain of the present utility model, the utility model
Institute's protection domain is to fit to the most wide scope consistent with principles disclosed herein and features of novelty.
Claims (7)
1. a kind of association response device of glyoxal oxidation synthesis glyoxylate, it includes：Reactor, nitric acid add pipe, circulating pump,
Gas-liquid reaction device, air intlet, reacting pipe, external heat exchanger, circulation water entrance, reflux condenser, cool brine turnover
Mouth, sample tap, glyoxalic acid outlet, tail gas absorber, it is characterised in that gas-liquid reaction device one end passes through circulating pump and reactor
Bottom is connected, and the other end of gas-liquid reaction device is connected by external heat exchanger with reactor top, the side of gas-liquid reaction device
Import and air communication, reactor, external heat exchanger, gas-liquid reaction device composition association response device realize glyoxal to acetaldehyde
The conversion reaction of acid.
2. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that institute
It is F that the nitric acid stated adds tubing matter4Or enamel material, its port is connected with homemade nitric acid at the uniform velocity Dropping feeder.
3. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that described
Gas-liquid reaction device be enamel, PP, F4Material, its port is connected with fluid accelerating attachment.
4. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that described
External heat exchanger be graphite, glass material heat exchanger, heat exchange area is 10-80m2。
5. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that described
Reflux condenser be coil pipe type glass condenser or graphite condenser, area is 1.5-15.0m2。
6. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that described
Air duct be PP materials, air intlet installs purifier additional.
7. a kind of association response device of glyoxal oxidation synthesis glyoxylate according to claim 1, it is characterised in that described
Tail gas absorber be PP materials, built-in spherical PE fillers or ripple packing, by 2-8 platforms absorption tower series connection turn into an absorption tower
Combination.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620590366.3U CN206276369U (en) | 2016-06-17 | 2016-06-17 | A kind of association response device of glyoxal oxidation synthesis glyoxylate |
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| CN201620590366.3U CN206276369U (en) | 2016-06-17 | 2016-06-17 | A kind of association response device of glyoxal oxidation synthesis glyoxylate |
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| Publication Number | Publication Date |
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| CN206276369U true CN206276369U (en) | 2017-06-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179150A (en) * | 2016-07-23 | 2016-12-07 | 河南新天地药业股份有限公司 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
-
2016
- 2016-06-17 CN CN201620590366.3U patent/CN206276369U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179150A (en) * | 2016-07-23 | 2016-12-07 | 河南新天地药业股份有限公司 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
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